CN105115943A - Gold seed growth based preparation method of terminal reflective optical fiber surface plasmon resonance sensor - Google Patents
Gold seed growth based preparation method of terminal reflective optical fiber surface plasmon resonance sensor Download PDFInfo
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- CN105115943A CN105115943A CN201510431719.5A CN201510431719A CN105115943A CN 105115943 A CN105115943 A CN 105115943A CN 201510431719 A CN201510431719 A CN 201510431719A CN 105115943 A CN105115943 A CN 105115943A
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Abstract
The invention relates to a gold seed growth based preparation method of a terminal reflective optical fiber surface plasmon resonance (SPR) sensor. The method includes: treating bare fiber by aminopropyltrimethoxysilane, then functionalizing the surface by -NH2; through electrostatic interaction with gold seed, adsorbing the gold seed to the bare fiber surface; in a film coating solution, letting the gold crystal rapidly grow into a dense gold film; sealing the end with silver so as to obtain an optical fiber SPR sensor. The method provided by the invention does not use large and expensive coating equipment, solves the defect of necessary use of a rotation device to ensure uniform thickness of an optical fiber cylindrical surface film in physical film coating, and the prepared sensor has high sensitivity to the surrounding environment, and has a sensitivity of 2054nm/RIU and 3980nm/RIU respectively in the refractive index range of 1.333-1.359 and 1.359-1.386, and also can be used for preparation of prism type SPR sensors, SPR sensors of various transmission modes and shapes and other gold film sensors.
Description
Technical field
The present invention relates to a kind of end reflection formula optical fiber surface plasmon resonance transducer production method based on the growth of gold kind, belong to surface plasma resonance spectrometer transducer production method.
Background technology
Optical-fiber type surface plasma resonance (Surfaceplasmonresonance, SPR) sensor, mutually doing quantitatively to detect with target molecule for monitoring molecule, being widely used in that medical diagnosis on disease, DNA hybridization and cell behavior are monitored, the field such as environment and food safety detection.It not only maintains the features such as conventional prism type spr sensor high sensitivity, unmarked real-time detection, and has its unique advantage, comprising: miniaturization, can resist Electromagnetic Interference, can realize remote recording etc.
Uniform metal film is the key that spr sensor has high sensitivity, excellent spr signal.Traditional optical fiber SPR sensor method of preparing uses expensive filming equipment, and by physical evaporation or sputtering method, the Cr that first optical fiber plate 2-3nm improves adhesiveness, then the noble metal plating 45-50nm provides free electron.But, be a cylinder for optical fiber, instead of the situation of glass sheet plane, in these physical coating methods, need to adopt complicated wheelwork to ensure the homogeneity of golden film on optical fiber cylinder.Gold plants the optical fiber preparation method of growth, need not use the wheelwork of this complexity, and it is with low cost, be easy to operation, in optical fiber SPR sensor preparation, have excellent application prospect.
Summary of the invention
The object of the invention is to provide a kind of end reflection formula optical fiber SPR sensor preparation method based on the growth of gold kind.This preparation method is simple to operate, with low cost, and the transducer sensitivity of preparation is high, good stability.The present invention is realized by the following technical programs.
A kind of end reflection formula optical fiber SPR sensor preparation method based on the growth of gold kind of the present invention, comprises the following steps:
A) predispersed fiber process: optical fiber is intercepted segment, the little section termination of optical fiber is as sensitive zones; Sensitive zones is soaked in the concentrated sulphuric acid, removes optical fiber surface polymkeric substance; After washed with de-ionized water, the sensitive zones removing polymkeric substance is soaked in 30min in 40%HF, removes optical fibre packages coating;
B) functional modification: step a) is soaked in Piranha washing lotion in the middle Fibre Optical Sensor region obtained, and optical fiber surface is modified rear taking-up by-OH, and by washed with de-ionized water, nitrogen dries up, and is placed in baking oven and is solidified by-the OH of optical fiber surface; Take out, be soaked in 6-12h in the methanol solution of 10% aminopropyl trimethoxysilane under normal temperature, now optical fiber surface is by-NH
2modify, take out, dry up with washed with methanol, nitrogen, be placed in baking oven by the-NH of optical fiber surface
2solidification;
C) gold is planted and is connected: by step b) surface that obtains is with firmly-NH
2the Fibre Optical Sensor region of group is soaked in gold and plants 8-12h in solution, and take out, washed with de-ionized water, nitrogen dries up;
D) plated film: by step c) the Fibre Optical Sensor region with gold kind that obtains is soaked in coating liquid, plated film reaction 5-8min in oscillator;
E) end face envelope silver: adopt silver mirror reaction, obtain end reflection formula spr sensor.
Described step a) in, optical fiber segment terminal length 0.5-2cm is sensitive zones.
Described step a) in, sensitive zones is soaked in the concentrated sulphuric acid of 85 DEG C.
Described step b) in, Piranha washing lotion is volume ratio is the concentrated sulphuric acid of 7:3 and the mixed liquor of hydrogen peroxide.
Described step b) in, it is 70-90 DEG C that optical fiber is soaked in Piranha wash temperature.
Described steps d) in, coating liquid is 0.1%HAuCl
4with 0.4mMNH
2the mixed liquor of OHHCl.
Described steps d) in, oscillator rotating speed is required to be 100rpm.
Method of the present invention also can be used for preparing the spr sensor of the various transmission mode such as prism-type spr sensor, on-line normalization formula, the spr sensor of the various shape such as U-shaped and other golden film sensors.
Compared with existing spr sensor preparation method, the invention has the advantages that: 1) of the present inventionly prepare spr sensor method, do not use relate in physical evaporation or splash method large-scale and the equipment of costliness, institute is convenient and simple in this way, and cost is low.
2) gold kind growth method of the present invention prepares optical-fiber type spr sensor, solves in physical coating and wheelwork must be used to ensure the thick uniform defect of optical fiber cylinder facial mask.
3) optical fiber SPR sensor prepared of the inventive method, obvious induction (see accompanying drawing 3) is had to surrounding environment refractive index, highly sensitive, be in 1.333-1.359 and 1.359-1.386 scope in refractive index respectively, sensitivity is 2054nm/RIU and 3980nm/RIU, sees accompanying drawing 4.
Accompanying drawing explanation
Fig. 1 gold is planted growth method and is prepared end reflection formula optical fiber surface plasmon resonance sensor process flow diagram.
Fig. 2 gold plants end reflection formula optical fiber SPR sensor photo in kind prepared by growth method.
Fig. 3 gold plants the reflectance spectrum of optical fiber SPR sensor in different refractivity solution prepared by growth method.
Fig. 4 gold plants optical fiber SPR sensor sensitivity investigation prepared by growth method.
Embodiment
Embodiment 1
After optical fiber being carried out removal polymkeric substance, the pre-service of removal clad, use deionized water and ethanol purge respectively, after nitrogen dries up, be soaked in 30min in the Piranha washing lotion (volume ratio is the concentrated sulphuric acid of 7:3 and the mixed liquor of hydrogen peroxide) of 70-90 DEG C, take out rear washed with de-ionized water, nitrogen dries up, and obtains the optical fiber surface that-OH modifies, be placed on 1h in 100 DEG C of baking ovens ,-the OH of optical fiber surface is solidified; Take out, be soaked in 8h in the methanol solution of 10% aminopropyl trimethoxysilane (APTMS) by with under the optical fiber normal temperature of-OH, take out rear washed with methanol, nitrogen dries up, and obtains-NH
2the optical fiber surface modified, is placed on 1h in 110 DEG C of baking ovens, by-the NH of optical fiber surface
2solidification.Traditional reduction of sodium citrate gold chloride legal system is adopted to be about the gold kind of 2.5nm for particle diameter, by above-mentioned-NH
2optical fiber after change is placed in gold and plants 8h-10h, and take out rear washed with de-ionized water, nitrogen dries up for subsequent use.Preparation coating liquid (0.1%HAuCl
4with 0.4mMNH
2the mixed liquor of OHHCl), be soaked in coating liquid by the optical fiber with gold kind, in oscillator, 100rpm reacts 7min, and optical fiber surface forms the golden film of one deck densification.End face envelope silver is carried out to golden film, the obtained end reflection formula optical fiber SPR sensor (see accompanying drawing 2) prepared based on gold kind growth method.
By the above-mentioned optical fiber SPR sensor obtained based on gold kind growth method by jiont treatments such as SMA905 to SPR spectrometer TT&C system.Set integral time, average time, smoothness, after signal stabilization, preserve half-light spectrum; Open light source, after signal stabilization, preserve reference spectra; Interface is adjusted to reflectivity patterns, the sensor of preparation is immersed in the water, action spectrum is superposed after signal stabilization, obtain the SPR of sensor in water and reflect spectrogram, equally, successively obtained sensor is immersed in acetonitrile, acetone, ethanol, hexane, n-propanol solution, obtain the SPR of sensor in above-mentioned several solns and reflect spectrogram.Origin software is mapped, and obtains the reflection spectrogram (see accompanying drawing 3) of spr sensor in the solution of above different refractivity prepared based on gold kind growth method; By calculating, the sensitivity of spr sensor respectively in the ranges of indices of refraction of 1.333-1.359 and 1.359-1.386 obtaining preparing based on gold kind growth method is 2054nm/RIU and 3980nm/RIU (see accompanying drawing 4).
Embodiment 2
After optical fiber being carried out removal polymkeric substance, the pre-service of removal clad, use deionized water and ethanol purge respectively, after nitrogen dries up, be soaked in 30min in the Piranha washing lotion (volume ratio is the concentrated sulphuric acid of 7:3 and the mixed liquor of hydrogen peroxide) of 70-90 DEG C, take out rear washed with de-ionized water, nitrogen dries up, and obtains the optical fiber surface that-OH modifies, be placed on 1h in 100 DEG C of baking ovens ,-the OH of optical fiber surface is solidified; Take out, be soaked in 6h in the methanol solution of 10% aminopropyl trimethoxysilane (APTMS) by with under the optical fiber normal temperature of-OH, take out rear washed with methanol, nitrogen dries up, and obtains-NH
2the optical fiber surface modified, is placed on 1h in 110 DEG C of baking ovens, by-the NH of optical fiber surface
2solidification.Traditional reduction of sodium citrate gold chloride legal system is adopted to be about the gold kind of 2.5nm for particle diameter, by above-mentioned-NH
2optical fiber after change is placed in gold and plants 8h, and take out rear washed with de-ionized water, nitrogen dries up for subsequent use.Preparation coating liquid (0.1%HAuCl
4with 0.4mMNH
2the mixed liquor of OHHCl), be soaked in coating liquid by the optical fiber with gold kind, in oscillator, 100rpm reacts 5min, 6min, 7min and 8min respectively.End face envelope silver is carried out to golden film, obtains the end reflection formula optical fiber SPR sensor under the different plated film times of preparing based on gold kind growth method.
According to the assay method in embodiment 1, measure the SPR reflection spectrogram of sensor in water that the plated film time is 5min, 6min, 7min and 8min respectively, mapped by origin software, and compare, learn: when the plated film time is 7min, the sensor spr signal obtained is best.
A kind of end reflection formula optical fiber surface plasmon resonance transducer production method based on the growth of gold kind that the present invention discloses and proposes, those skilled in the art are by using for reference present disclosure, the links such as suitable change condition and process route realize, although method of the present invention and technology of preparing are described by preferred embodiment, person skilled obviously can change Method and Technology route as herein described or reconfigure not departing from content of the present invention, spirit and scope, realizes final technology of preparing.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are deemed to be included in spirit of the present invention, scope and content.
Claims (8)
1., based on an end reflection formula optical fiber surface plasmon resonance transducer production method for gold kind growth, it is characterized in that comprising the following steps:
A) predispersed fiber process: optical fiber is intercepted segment, the little section termination of optical fiber is as sensitive zones; Sensitive zones is soaked in the concentrated sulphuric acid, removes optical fiber surface polymkeric substance; After washed with de-ionized water, the sensitive zones removing polymkeric substance is soaked in 30min in 40%HF, removes optical fibre packages coating;
B) functional modification: step a) is soaked in Piranha washing lotion in the middle Fibre Optical Sensor region obtained, and optical fiber surface is modified rear taking-up by-OH, and by washed with de-ionized water, nitrogen dries up, and is placed in baking oven and is solidified by-the OH of optical fiber surface; Take out, be soaked in 6-12h in the methanol solution of 10% aminopropyl trimethoxysilane under normal temperature, now optical fiber surface is by-NH
2modify, take out, dry up with washed with methanol, nitrogen, be placed in baking oven by the-NH of optical fiber surface
2solidification;
C) gold is planted and is connected: by step b) surface that obtains is with firmly-NH
2the Fibre Optical Sensor region of group is soaked in gold and plants 8-12h in solution, and take out, washed with de-ionized water, nitrogen dries up;
D) plated film: by step c) the Fibre Optical Sensor region with gold kind that obtains is soaked in coating liquid, plated film reaction 5-8min in oscillator;
E) end face envelope silver: adopt silver mirror reaction, obtain end reflection formula spr sensor.
2. the method for claim 1, in it is characterized in that described step a), optical fiber segment terminal length 0.5-2cm is sensitive zones.
3. the method for claim 1, in it is characterized in that described step a), sensitive zones is soaked in the concentrated sulphuric acid of 85 DEG C.
4. the method for claim 1, is characterized in that described step b) in, Piranha washing lotion is volume ratio is the concentrated sulphuric acid of 7:3 and the mixed liquor of hydrogen peroxide.
5. the method for claim 1, is characterized in that described step b) in, it is 70-90 DEG C that optical fiber is soaked in Piranha wash temperature.
6. the method for claim 1, is characterized in that described steps d) in, coating liquid is 0.1%HAuCl
4with 0.4mMNH
2the mixed liquor of OHHCl.
7. the method for claim 1, is characterized in that described steps d) in, oscillator rotating speed is required to be 100rpm.
8. the method for claim 1 is used for preparing prism-type spr sensor, the spr sensor of various transmission mode, the spr sensor of various shape and other golden film sensors.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106896087A (en) * | 2017-03-31 | 2017-06-27 | 丁利 | The preparation method of the surface plasma resonance instrument chip based on hyperbranched amphion polymethyl base cysteine modified |
| CN109239050A (en) * | 2018-09-17 | 2019-01-18 | 中科院合肥技术创新工程院 | Hollow-core fiber SERS probe preparation method and harmful gas detection system |
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| CN101190829A (en) * | 2006-11-29 | 2008-06-04 | 河南农业大学 | Method for preparing optical fiber SPR sensor gold film by microwave radiation assisted chemical plating |
| CN102507503A (en) * | 2011-10-24 | 2012-06-20 | 天津大学 | Fiber surface plasmon resonance glucose sensor with temperature self-compensation |
| CN102608068A (en) * | 2012-03-09 | 2012-07-25 | 天津理工大学 | Photonic crystal fiber SPR (Surface Plasmon Resonance) sensing model with novel structure |
| CN102621104A (en) * | 2012-03-15 | 2012-08-01 | 电子科技大学 | Graphene film sensitized D-shaped optical fiber surface plasmon resonance (SPR) sensor and preparation method thereof |
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2015
- 2015-07-21 CN CN201510431719.5A patent/CN105115943A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101038253A (en) * | 2006-10-23 | 2007-09-19 | 北京赛德创生物技术有限公司 | Micro-prisms array SPR biosensor component |
| CN101190829A (en) * | 2006-11-29 | 2008-06-04 | 河南农业大学 | Method for preparing optical fiber SPR sensor gold film by microwave radiation assisted chemical plating |
| CN102507503A (en) * | 2011-10-24 | 2012-06-20 | 天津大学 | Fiber surface plasmon resonance glucose sensor with temperature self-compensation |
| CN102608068A (en) * | 2012-03-09 | 2012-07-25 | 天津理工大学 | Photonic crystal fiber SPR (Surface Plasmon Resonance) sensing model with novel structure |
| CN102621104A (en) * | 2012-03-15 | 2012-08-01 | 电子科技大学 | Graphene film sensitized D-shaped optical fiber surface plasmon resonance (SPR) sensor and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106896087A (en) * | 2017-03-31 | 2017-06-27 | 丁利 | The preparation method of the surface plasma resonance instrument chip based on hyperbranched amphion polymethyl base cysteine modified |
| CN106896087B (en) * | 2017-03-31 | 2019-04-23 | 丁利 | The preparation method of surface plasma resonance instrument chip based on hyperbranched amphoteric ion polymethyl base cysteine modified |
| CN109239050A (en) * | 2018-09-17 | 2019-01-18 | 中科院合肥技术创新工程院 | Hollow-core fiber SERS probe preparation method and harmful gas detection system |
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Application publication date: 20151202 |